CN110828089B - Neodymium-iron-boron magnet material, raw material composition, preparation method and application - Google Patents

Neodymium-iron-boron magnet material, raw material composition, preparation method and application Download PDF

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CN110828089B
CN110828089B CN201911150975.1A CN201911150975A CN110828089B CN 110828089 B CN110828089 B CN 110828089B CN 201911150975 A CN201911150975 A CN 201911150975A CN 110828089 B CN110828089 B CN 110828089B
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boron magnet
magnet material
iron boron
neodymium iron
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CN110828089A (en
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付刚
黄佳莹
黄吉祥
权其琛
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Fujian Jinlong Rare Earth Co ltd
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Xiamen Tungsten Co Ltd
Fujian Changting Jinlong Rare Earth Co Ltd
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Priority to CN201911150975.1A priority Critical patent/CN110828089B/en
Publication of CN110828089A publication Critical patent/CN110828089A/en
Priority to JP2021552780A priority patent/JP7220301B2/en
Priority to EP20890034.0A priority patent/EP3940722B1/en
Priority to DK20890034.0T priority patent/DK3940722T3/en
Priority to US17/600,105 priority patent/US20220285059A1/en
Priority to KR1020217037134A priority patent/KR102527787B1/en
Priority to PCT/CN2020/100587 priority patent/WO2021098224A1/en
Priority to ES20890034T priority patent/ES2984871T3/en
Priority to TW109139812A priority patent/TWI751789B/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0573—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes obtained by reduction or by hydrogen decrepitation or embrittlement
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

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  • Power Engineering (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses a neodymium iron boron magnet material, a raw material composition, a preparation method and application. The raw material composition of the neodymium iron boron magnet material comprises the following components in percentage by mass: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; b: 0.9-1.2%; fe: 64-69.2%, wherein the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material. The residual magnetism and the coercive force of the obtained neodymium iron boron magnet material are still high under the condition that heavy rare earth elements are not added.

Description

Neodymium-iron-boron magnet material, raw material composition, preparation method and application
Technical Field
The invention particularly relates to a neodymium iron boron magnet material, a raw material composition, a preparation method and application.
Background
By Nd2Fe14The neodymium iron boron (NdFeB) magnet material with the B as the main component has higher remanence, coercive force and maximum magnetic energy product, has excellent comprehensive magnetic performance, and is applied to the aspects of wind power generation, new energy automobiles, variable frequency household appliances and the like. At present, the rare earth component in the neodymium iron boron magnet material in the prior art is mainly neodymium, and only a small amount of praseodymium is contained. Although there are few reports in the prior art that a part of neodymium is replaced by praseodymium to improve the performance of the magnet material, the improvement degree is limited, and the improvement is not significant. On the other hand, in the prior art, the neodymium iron boron magnet material with good coercive force and remanence performance also needs to depend on a large amount of addition of heavy rare earth elements, and the cost is expensive.
Disclosure of Invention
The invention aims to solve the technical problem that the coercive force and remanence of a magnet material can not be obviously improved after neodymium is replaced by part of praseodymium in the neodymium iron boron magnet material in the prior art. The neodymium iron boron magnet material, the raw material composition, the preparation method and the application are provided. The neodymium iron boron magnet material disclosed by the invention has the advantages that the content of praseodymium and copper is simultaneously increased, the defect that the coercive force cannot be obviously improved even if praseodymium is increased or copper is increased independently in the prior art can be overcome, and the obtained neodymium iron boron magnet material has high remanence and coercive force.
At present, it is generally considered in the prior art that the wettability can be increased by adding a small amount of copper to the neodymium iron boron magnet material. However, through a large number of experiments, the inventor finds that RECu appears after a specific content of praseodymium and a specific content of copper are combined2RECu and RE6Fe13Cu and other non-magnetic phases, wherein RE refers to neodymium element and praseodymium element, and the occurrence of the non-magnetic phases effectively isolates the magnetic coupling effect among crystal grains, and simultaneously can also improve the definition degree of a crystal boundary and optimize the crystal boundary phase, so that the performance of the neodymium iron boron magnet is further improved.
The invention solves the technical problems through the following technical scheme.
The invention also provides a raw material composition of the neodymium iron boron magnet material, which comprises the following components in percentage by mass:
r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent;
Cu：≥0.35％；
B：0.9～1.2％；
fe: 64-69.2%, wherein the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the content of Pr is preferably 17.15 to 26%, for example, 17.15%, 18.15%, 19.15%, 20.15%, 20.85%, 21.15%, 22.15%, 23.15%, 24.15%, 25.15% or 26%, where the percentage is mass% of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the content of Nd is preferably less than 15%, more preferably 4 to 13%, for example, 4%, 5.85%, 6.85%, 7.85%, 8.85%, 9.85%, 10.65%, 10.85%, 11.35%, 12.35%, or 12.85%, where the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the content of R' is, for example, 29.5%, 30%, 30.5%, 31%, 31.5%, or 32%, and the percentage refers to the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, said R' preferably further comprises other rare earth elements other than Pr and Nd, such as Y.
In the present invention, the R' preferably further includes RH, which is a heavy rare earth element, and the kind of RH preferably includes one or more of Dy, Tb and Ho, and more preferably Dy and/or Tb.
Wherein the mass ratio of RH and R' is preferably less than 0.253, preferably 0-0.07, such as 0, 1/32, 2/32, 2/31, 1.5/32, 2/32 or 1.5/31.
The content of RH is preferably 1 to 2.5%, for example, 1%, 1.5%, or 2%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
When the RH contains Tb, the content of Tb is preferably 0.5 to 2%, for example, 0.7%, 0.8%, 0.9%, 1%, 1.5%, 1.8%, 1.9%, or 2%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
When Dy is contained in the RH, the content of Dy is preferably 1% or less, more preferably 0.3% or less, for example, 0.1%, 0.2%, or 0.3%, and the percentage means a mass percentage based on the total mass of the raw material composition of the neodymium iron boron magnet material.
When the RH contains Ho, the content of Ho may be a content conventional in the art, for example, 0.8 to 2%, preferably 1%, and the percentage refers to a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the content of Cu is preferably 0.35to 1.3%, for example, 0.35%, 0.4%, 0.45%, 0.5%, 0.6%, 0.65%, 0.7%, 0.8%, 0.85%, 0.9%, 0.95%, 1%, 1.05%, 1.1%, or 1.2%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the content of B is preferably 0.95 to 1.2%, for example, 0.985%, 1%, 1.1% or 1.2%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the content of Fe is preferably 64.8 to 69.2%, for example, 64.914%, 64.965%, 65.065%, 65.085%, 65.135%, 65.365%, 65.405%, 65.485%, 65.54%, 65.615%, 65.665%, 65.715%, 65.815%, 65.865%, 65.915%, 66.015%, 66.035%, 66.045%, 66.215%, 66.23%, 66.265%, 66.315%, 66.465%, 66.445%, 66.545%, 66.615%, 66.715%, 66.815%, 66.865%, 67.145%, 67.165%, 67.415%, 67.615%, 67.915%, 68.015%, 68.295%, 68.565% or 69.165%, which is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the raw material composition of the neodymium iron boron magnet material preferably further includes Al.
The content of Al is preferably 3% or less, more preferably 0.5% or less, for example, 0.02%, 0.03%, 0.1%, 0.2%, 0.25%, 0.3%, 0.4%, 0.45%, 0.46%, or 0.48%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the raw material composition of the neodymium iron boron magnet material preferably further includes Ga.
The content of Ga is preferably less than 1%, more preferably 0.05 to 0.6%, for example, 0.1%, 0.15%, 0.18%, 0.2%, 0.24%, 0.25%, 0.3%, 0.4% or 0.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the raw material composition of the neodymium iron boron magnet material preferably further includes Zr.
The content of Zr is preferably less than 0.3%, for example, 0.1%, 0.2%, 0.22%, 0.25%, 0.26%, 0.27%, 0.28%, 0.29%, or 0.3%, and more preferably 0.25 to 0.3%, where the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the raw material composition of the neodymium iron boron magnet material preferably further includes Co.
The content of Co is preferably 0.2 to 1.5%, for example, 0.2% or 1%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the raw material composition of the neodymium iron boron magnet material may further include other elements commonly used In the art, such as one or more of Zn, Ag, In, Sn, V, Cr, Mo, Ta, Hf, and W.
The content of Zn may be a content conventionally used in the art, and is preferably less than 0.1%, more preferably 0.04-0.08%, such as 0.04%, 0.05% or 0.08%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
The content of Mo may be a content conventionally used in the art, and is preferably less than 0.1%, more preferably 0.01 to 0.08%, such as 0.04%, 0.05% or 0.08%, where the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.2%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-68%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.2%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.2%; more preferably, the R' further comprises RH, wherein the RH is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1-2.5%; the RH is preferably Dy and/or Tb, wherein the Tb content is preferably 0.5-2%, and the Dy content is preferably less than 1%; the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; ga: less than or equal to 0.42 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; ga: less than or equal to 0.42 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; ga: less than or equal to 0.42 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the raw material composition of the neodymium iron boron magnet material preferably comprises the following components by mass percent: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; ga: less than or equal to 0.42 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.15-26%; more preferably, the content of Cu is 0.35-1.2%; more preferably, the R' further comprises RH, wherein the RH is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1-2.5%; the RH is preferably Dy and/or Tb, wherein the Tb content is preferably 0.5-2%, and the Dy content is preferably less than 1%; the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
In the invention, the percentage is the mass percentage of each component in the total mass of the raw material composition of the neodymium iron boron magnet material.
The invention also provides a preparation method of the neodymium iron boron magnet material, which is prepared by adopting the raw material composition of the neodymium iron boron magnet material.
In the present invention, the preparation method preferably comprises the steps of: and (3) carrying out fusion casting, hydrogen cracking, forming, sintering and aging treatment on the molten liquid of the raw material composition of the neodymium iron boron magnet material.
In the present invention, the melt of the raw material composition of the neodymium iron boron magnet material may be prepared by a method conventional in the art, for example: smelting in a high-frequency vacuum induction smelting furnace. The vacuum degree of the smelting furnace can be 5 multiplied by 10-2Pa. The temperature of the smelting can be below 1500 ℃.
In the present invention, the casting operation and conditions may be those conventional in the art, for example, in an Ar gas atmosphere (e.g., 5.5X 10)4Pa of Ar gas atmosphere) at 10 deg.f2DEG C/sec-104Cooling at a rate of DEG C/sec.
In the present invention, the hydrogen decrepitation may be performed under the conventional conditions. For example, the treatment of hydrogen absorption, dehydrogenation and cooling is carried out.
Wherein the hydrogen absorption can be carried out under the condition that the hydrogen pressure is 0.15 MPa.
Wherein the dehydrogenation is carried out under a condition of raising the temperature while evacuating.
In the present invention, the hydrogen may be broken and then pulverized by a conventional method in the art. The comminution process may be a comminution process conventional in the art, such as jet milling. The jet milling is preferably carried out under a nitrogen atmosphere having an oxidizing gas content of 150ppm or less. The oxidizing gas refers to oxygen or moisture content. The pressure of a crushing chamber for crushing by the jet mill is preferably 0.38 MPa; the jet mill pulverizing time is preferably 3 h.
After the pulverization, a lubricant such as zinc stearate may be added to the powder by a conventional method in the art. The amount of the lubricant added may be 0.10 to 0.15%, for example, 0.12% by weight of the mixed powder.
In the present invention, the operation and conditions of the forming may be those conventional in the art, such as a magnetic field forming method or a hot press hot deformation method.
In the present invention, the operation and conditions of the sintering may be those conventional in the art. For example, under vacuum conditions (e.g. at 5X 10)-3Pa, vacuum), preheating, sintering and cooling.
Wherein the preheating temperature is usually 300-600 ℃. The preheating time is usually 1-2 h. Preferably the preheating is for 1h at a temperature of 300 ℃ and 600 ℃ each.
Wherein, the sintering temperature is preferably 1030-1080 ℃, for example 1040 ℃.
The sintering time may be conventional in the art, e.g., 2 hours.
Wherein Ar gas can be introduced before cooling to ensure that the gas pressure reaches 0.1 MPa.
In the present invention, after the sintering and before the aging treatment, a grain boundary diffusion treatment is preferably further performed.
The operation and conditions for grain boundary diffusion can be those conventional in the art. For example, a Tb-containing substance and/or a Dy-containing substance may be deposited on the surface of the neodymium-iron-boron magnet material by vapor deposition, coating, or sputtering, and then subjected to diffusion heat treatment.
The Tb containing substance may be Tb metal, a Tb containing compound, such as a Tb containing fluoride or an alloy.
The Dy-containing substance may be Dy metal, a Dy-containing compound, such as a fluoride containing Dy, or an alloy.
The temperature of the diffusion heat treatment may be 800-.
The diffusion heat treatment time may be 12-48h, for example 24 h.
In the invention, in the aging treatment, the temperature of the secondary aging treatment is preferably 520-650 ℃, for example 550 ℃.
In the present invention, in the secondary aging treatment, the heating rate of the temperature to 550 to 650 ℃ is preferably 3to 5 ℃/min. The starting point of the warming may be room temperature.
In the present invention, the room temperature means 25 ℃. + -. 5 ℃.
The invention also provides a neodymium iron boron magnet material which is prepared by adopting the preparation method.
The invention provides a neodymium iron boron magnet material which comprises the following components in percentage by mass:
r': 29.4-32.6%, wherein R' comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent;
Cu：≥0.34％；
B：0.9～1.2％；
Fe：64～69.2％；
the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the present invention, the content of Pr is preferably 17.14 to 26.1%, for example, 17.149%, 17.15%, 17.154%, 18.15%, 18.152%, 18.154%, 18.155%, 19.15%, 19.152%, 19.154%, 19.155%, 19.159%, 20.13%, 20155%, 20.16%, 21.157%, 22.15%, 22.151%, 22.152%, 22.1555%, 23.15%, 24.151%, 24.152%, 24.155%, 24.157%, 24.158%, 25.15%, 25.152%, 25.153%, 25.156% or 26.01%, where the percentage is a mass percentage of the total mass of the neodymium iron boron magnet material.
In the present invention, the content of Nd is preferably 15% or less, more preferably 4 to 13%, for example, 4.02%, 5.847%, 5.84%, 85.849%, 5.85%, 5.851%, 5.852%, 5.853%, 5.854%, 6.851%, 6.852%, 6.853%, 7.85%, 8.846%, 8.847%, 8.85%, 8.851%, 8.852%, 8.853%, 9.85%, 9.851%, 10.844%, 10.846%, 10.849%, 11.349%, 11.384%, 12.341%, 12.345%, 12.348%, 12.35%, 12.351%, 12.364%, 12.791%, 12.802% or 12.849%, which is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the present invention, the ratio of the total mass of the Nd and the R' is preferably less than 0.5, more preferably 0.1 to 0.45, for example, 0.1, 0.12, 0.13, 0.18, 0.2, 0.21, 0.23, 0.24, 0.25, 0.26, 0.27, 0.3, 0.31, 0.37, 0.38, 0.4, 0.41 or 0.42.
In the present invention, the content of R' is preferably 29.49 to 32.53%, for example, 29.495%, 29.501%, 30.003%, 30.004%, 30.03%, 30.441%, 30.517%, 30.518%, 30.957%, 30.98%, 31%, 31.006%, 31.0065%, 31.009%, 31.011%, 31.012%, 31.013%, 31.498%, 31.504%, 31.539%, 31.946%, 31.972%, 31.977%, 31.995%, 31.999%, 32%, 32.001%, 32.013%, 32.015%, 32.021%, 32.022%, 32.023, 32.024%, 32.025%, 32.026%, 32.027%, 32.04%, 32.043%, 32.437% or 32.521%, and the percentage is a mass percentage of the total mass of the neodymium iron boron magnet material.
In the present invention, said R' preferably further comprises other rare earth elements other than Pr and Nd, such as Y.
In the present invention, R' preferably further includes RH, which is a heavy rare earth element, and the kind of RH preferably includes one or more of Dy, Tb, and Ho, and more preferably Dy and/or Tb.
Wherein, the mass ratio of the RH and the R' is preferably less than 0.253, preferably 0-0.07, such as 1.01/32.015, 1.02/30.517, 1.02/32.021, 1.02/32.023, 1.02/32.024, 1.02/32.024, 1.02/32.025, 1.02/32.025, 1.02/32.026, 1.03/32.04, 1.04/32.043, 1.432/32.437, 1.46/30.441, 1.47/31.972, 1.48/31.977, 1.5/32, 1.52/32.521, 1.98/30.98, 1.99/31.995, 1/31.999, 1/32, 2.01/31.011, 2.01/31.013, 2.01/32.013, 2.02/32.022, 2.02/32.027, 2/31 or 2/31.012.
The content of RH is preferably 1 to 2.5%, for example, 1%, 1.01%, 1.02%, 1.03%, 1.04%, 1.432%, 1.46%, 1.47%, 1.48%, 1.5%, 1.52%, 1.98%, 1.99%, 2%, 2.01%, or 2.02%, and the percentage is a mass percentage of the total mass of the neodymium iron boron magnet material.
When the RH contains Tb, the content of Tb is preferably 0.5 to 2wt%, for example, 0.7%, 0.72%, 0.82%, 0.9%, 0.91%, 1%, 1.02%, 1.47%, 1.48%, 1.5%, 1.81%, 1.88%, 1.89%, 1.9%, 1.91%, or 2.01%, and the percentage is a mass percentage of the total mass of the neodymium iron boron magnet material.
When Dy is contained in the RH, the content of Dy is preferably 0.5wt% or less, for example, 0.1%, 0.2%, 0.21%, 0.3%, 0.31%, or 0.312%, by mass percentage in the neodymium iron boron magnet material.
When the RH includes Ho, the content of Ho may be a content conventional in the art, and is usually 0.8 to 2%, for example, 0.98%, 0.99% or 1%, where the percentage refers to the mass percentage in the neodymium iron boron magnet material.
In the present invention, the Cu content is preferably 0.34 to 1.3%, for example, 0.341%, 0.41%, 0.452%, 0.47%, 0.502%, 0.51%, 0.52%, 0.598%, 0.62%, 0.648%, 0.649%, 0.701%, 0.702%, 0.71%, 0.78%, 0.79%, 0.795%, 0.806%, 0.81%, 0.852%, 0.89%, 0.901%, 0.903%, 0.91%, 0.92%, 0.948%, 1.021%, 1.05%, 1.08%, 1.101%, 1.103%, 1.12%, 1.18%, 1.19%, 1.202%, or 1.21%, and the percentage is a mass percentage in the neodymium iron boron magnet material.
In the present invention, the content of B is preferably 0.95 to 1.2%, for example, 0.983%, 0.984%, 0.985%, 0.988%, 0.989%, 1.02% or 1.19%, and the percentage refers to the mass percentage of the neodymium iron boron magnet material.
In the present invention, the content of Fe is preferably 64.8 to 69.2%, for example, 64.965%, 65.031%, 65.095%, 65.155%, 65.204%, 65.36%, 65.4%, 65.458%, 65.525%, 65.626%, 65.63%, 65.686%, 65.817%, 65.8395, 65.869%, 65.909%, 65.963%, 65.994%, 65.995%, 66.039%, 66.04%, 66.099%, 66.157%, 66.218%, 66.267%, 66.364%, 66.377%, 66.427%, 66.437%, 66.52%, 66.605%, 66.671%, 66.8075%, 66.81%, 66.87%, 67.095%, 67.12%, 67.137%, 67.457%, 67.578%, 67.996%, 68.302%, 68.556% or 69.181%, and the percentage refers to the mass percentage in the neodymium iron boron magnet material.
In the present invention, the neodymium iron boron magnet material preferably further includes Al.
In the present invention, the content of Al is preferably 0.5% or less, more preferably 0.03 to 0.5wt%, for example, 0.01%, 0.02%, 0.03%, 0.1%, 0.102%, 0.12%, 0.2%, 0.21%, 0.24%, 0.25%, 0.29%, 0.3%, 0.31%, 0.38%, 0.4%, 0.42%, 0.45%, 0.46% or 0.48%, and the percentage refers to the mass percentage in the neodymium iron boron magnet material.
In the present invention, the neodymium iron boron magnet material preferably further includes Zr.
In the present invention, the content of Zr is preferably 0.05 to 0.31wt%, such as 0.1%, 0.21%, 0.22%, 0.25%, 0.251%, 0.252%, 0.261%, 0.272%, 0.28%, 0.281%, 0.282%, 0.291%, 0.3%, or 0.301%, and more preferably 0.25 to 0.31%, in percentage by mass of each component based on the total mass of the ndfeb magnet material.
In the present invention, the neodymium iron boron magnet material preferably further includes Ga.
Wherein, the content of the Ga is preferably less than 0.51%, preferably 0.1-0.51%, such as 0.1%, 0.101%, 0.102%, 0.11%, 0.12%, 0.152%, 0.18%, 0.2%, 0.202%, 0.24%, 0.25%, 0.251%, 0.302%, 0.401% or 0.501%, and the percentage is the percentage of the mass of each component in the total mass of the ndfeb magnet material.
In the present invention, the neodymium iron boron magnet material preferably further includes Co.
The content of Co is preferably 0.2-1.5%, for example 0.2% or 1%, and the percentage is the percentage of the mass of each component in the total mass of the neodymium iron boron magnet material.
In the present invention, the neodymium iron boron magnet material usually further includes O.
Wherein, the content of O is preferably below 0.13 percent, and the percentage is the percentage of the mass of each component in the total mass of the neodymium iron boron magnet material.
In the present invention, the neodymium iron boron magnet material may further include other elements commonly known In the art, such as one or more of Zn, Ag, In, Sn, V, Cr, Nb, Ti, Mo, Ta, Hf and W.
The content of Zn may be a content conventional in the art, and is preferably 0.02 to 0.08, for example, 0.03%, 0.04%, or 0.07%, where the percentage is the percentage of the mass of each component in the total mass of the neodymium iron boron magnet material.
The content of Mo may be a content conventional in the art, and is preferably 0.01 to 0.08%, for example, 0.03%, 0.06%, or 0.07%, where the percentage is the percentage of the mass of each component in the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; al: less than or equal to 0.5 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.2%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.34%; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.2%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; al: less than or equal to 0.5 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.2%; more preferably, the R' further comprises RH, wherein the RH is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1-2.5%; the RH is preferably Dy and/or Tb, wherein the Tb content is preferably 0.5-2%, and the Dy content is preferably less than 1%; the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; ga: less than or equal to 0.42 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; al: less than or equal to 0.5 percent; ga: less than or equal to 0.42 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; ga: less than or equal to 0.42 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.3%; more preferably, R' further includes RH, which is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1 to 2.5%, and the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the neodymium iron boron magnet material preferably comprises the following components in percentage by mass: r': 29.4-32.6%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent; cu: not less than 0.34%; al: less than or equal to 0.5 percent; ga: less than or equal to 0.42 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; more preferably, the content of Pr is 17.14-26.1%; more preferably, the content of Cu is 0.35-1.3%; more preferably, the R' further comprises RH, wherein the RH is a heavy rare earth element, and the content of the heavy rare earth element is preferably 1-2.5%; the RH is preferably Dy and/or Tb, wherein the Tb content is preferably 0.5-2%, and the Dy content is preferably less than 1%; the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material.
In the invention, the percentage is the mass percentage of each component in the total mass of the neodymium iron boron magnet material.
The invention also provides a neodymium iron boron magnet material, in the inter-crystal triangular area of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element in the inter-crystal triangular area is Q1; at the grain boundary of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element at the grain boundary is Q2; wherein Q1 is less than Q2, and Q2 is more than or equal to 0.1;
preferably, the composition of the ndfeb magnet material is as described above.
In the present invention, the grain boundary refers to a boundary between two crystal grains, and the intercrystalline triangular region refers to a void formed by three or more crystal grains.
The invention also provides application of the neodymium iron boron magnet material in a motor as an electronic element.
In the invention, the motor is preferably a new energy automobile driving motor, an air conditioner compressor or an industrial servo motor, a wind driven generator, an energy-saving elevator or a loudspeaker assembly.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: according to the neodymium iron boron magnet material, the content of praseodymium and copper is simultaneously increased, so that the grain boundary phase is clearer, and the remanence and the coercive force of the obtained neodymium iron boron magnet material are higher.
Drawings
Fig. 1 is a distribution diagram of elements Pr, Nd, Cu, Ti, Co and O formed by FE-EPMA surface scanning of the neodymium iron boron magnet material prepared in example 10.
Fig. 2 is an element distribution diagram at the grain boundary of the neodymium-iron-boron magnet material in example 10, and fig. 1 is a point taken by quantitative analysis in the grain boundary.
Fig. 3 is an elemental distribution diagram of the intercrystalline triangular space of the neodymium-iron-boron magnet material in example 10, and fig. 1 is a point taken for quantitative analysis in the intercrystalline triangular space.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The raw material compositions of the neodymium iron boron magnet materials in each example and comparative example are shown in table 1 below.
TABLE 1
Figure BDA0002283533230000151
Figure BDA0002283533230000161
Example 1
The preparation method of the neodymium iron boron magnet material comprises the following steps:
(1) and (3) casting: according to the formulation shown in Table 1, the prepared raw materials were put into a crucible made of alumina, and placed in a high-frequency vacuum induction melting furnace at 5X 10-2Vacuum melting is carried out at a temperature of 1500 ℃ or lower in a vacuum of Pa. Ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(2) Hydrogen crushing and crushing: vacuumizing the smelting furnace in which the quenching alloy is placed at room temperature, introducing hydrogen with the purity of 99.9% into the hydrogen cracking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, vacuumizing while heating, fully dehydrogenating, cooling, and taking out the powder after hydrogen cracking and crushing.
(3) A micro-grinding process: the powder after hydrogen crushing was pulverized by jet milling for 3 hours under a nitrogen atmosphere having an oxidizing gas content of 150ppm or less at a pressure in the pulverization chamber of 0.38MPa to obtain a fine powder. The oxidizing gas refers to oxygen or moisture.
(4) Adding zinc stearate into the powder crushed by the jet mill, wherein the adding amount of the zinc stearate is 0.12 percent of the weight of the mixed powder, and then fully mixing the zinc stearate and the mixed powder by using a V-shaped mixer.
(5) Magnetic field forming process: using a magnetic field forming machine of a perpendicular orientation type, in an orientation magnetic field of 1.6T, at 0.35ton/cm2The powder added with zinc stearate was once formed into a cube with a side length of 25mm under the molding pressure of (1), and demagnetized in a magnetic field of 0.2T after the primary molding. The molded article after the primary molding was sealed so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm2Secondary forming is performed under pressure of (1).
(6) And (3) sintering: the molded bodies were transferred to a sintering furnace and sintered at 5X 10-3Pa at 300 deg.C and 600 deg.C for 1 hr, sintering at 1040 deg.C for 2 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(7) And (3) aging treatment process: the sintered body was heat-treated in high-purity Ar gas at 550 ℃ for 3 hours, cooled to room temperature, and taken out.
The preparation processes of examples 2 to 42 and comparative examples 45 to 48 are the same as example 1.
Examples 43 and 44 preparation Process Using Tb grain boundary diffusion method
The raw material compositions of nos. 12 and 16 in table 1 were subjected to grain boundary diffusion and aging treatment, after preparing a sintered body according to the preparation of the sintered body of example 1. The aging treatment process is the same as that of the example 1, and the treatment process of grain boundary diffusion is as follows:
processing the sintered body into a magnet with the diameter of 20mm and the sheet thickness of less than 7mm, wherein the thickness direction is the magnetic field orientation direction, cleaning the surface, respectively using a raw material prepared from Tb fluoride, spraying and coating the whole surface of the magnet, drying the coated magnet, sputtering metal attached with Tb on the surface of the magnet in a high-purity Ar gas atmosphere, and performing diffusion heat treatment at the temperature of 850 ℃ for 24 hours. And cooling to room temperature.
Effect example 1
The magnetic properties and components of the neodymium iron boron magnet materials prepared in the examples and the comparative examples are measured, and the crystalline phase structure of the magnet is observed by FE-EPMA.
(1) Evaluation of magnetic Properties: the sintered magnet is subjected to magnetic property detection by using an NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China measurement institute. The following table 2 shows the results of magnetic property measurements.
TABLE 2
Figure BDA0002283533230000181
Figure BDA0002283533230000191
(2) Component determination: each component was measured using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES). The following table 3 shows the results of component detection.
TABLE 3
Figure BDA0002283533230000192
Figure BDA0002283533230000201
Figure BDA0002283533230000211
(3) FE-EPMA detection: the vertical orientation surface of the sintered magnet was polished in example 10 and examined by a field emission electron probe microanalyzer (FE-EPMA) (JEOL 8530F). Firstly, the distribution of elements such as Pr, Cu, B, Fe, Co, O and the like in a magnet is determined through FE-EPMA surface scanning, and then the content of the elements such as Pr, Cu, O and the like in a key phase is determined through FE-EPMA single-point quantitative analysis under the test conditions of 15kv of acceleration voltage and 50nA of probe beam current.
The magnetic steel prepared by the formula mainly analyzes elements Pr, Nd, Cu, Ti, Co and O by adopting a field emission electron probe microanalyzer (FE-EPMA), and quantitatively analyzes elements at a crystal boundary and an intercrystalline triangular region as shown in figure 1. Wherein: the grain boundary refers to the boundary between two grains, and the intercrystalline triangular region refers to the gap formed by three or more grains.
As shown in fig. 2, in order to obtain the distribution of elements at the grain boundary of the neodymium-iron-boron magnet material of example 10, the elements Pr and Nd are mainly distributed in the main phase, part of the rare earth also appears at the grain boundary, the elements Cu and Zr are distributed at the grain boundary, and the quantitative results of the elements at the grain boundary at the point marked by 1 in fig. 2 are shown in the following table 4:
TABLE 4
Figure BDA0002283533230000212
As can be seen from the above data, Pr and Nd exist in the form of a rare earth-rich phase and oxides in the grain boundaries, alpha-Pr and alpha-Nd, Pr2O3，Nd2O3And NdO, Cu occupying a certain content of about 28 wt.% except at the grain boundaries outside the main phase, for example 28.6 wt.% in the present example. Zr is used as a high-melting-point element to be dispersed and distributed in the whole area, the effective distribution of Cu combines the combined action of Pr, the wettability of a crystal boundary is improved, the crystal defect is repaired, and the performance of the magnet is improved.
As shown in fig. 3, for the distribution of the elements in the inter-granular triangular regions of the neodymium-iron-boron magnet material of example 10, the quantitative results of the points marked with 1 in fig. 3 for the elements in the inter-granular triangular regions are shown in table 5 below:
TABLE 5
Figure BDA0002283533230000213
Figure BDA0002283533230000221
In the intercrystalline triangular region, Pr and Nd elements are distributed and in the intercrystalline triangular region, in a high-Pr formula, it is clearly found that Pr and Nd in the intercrystalline triangular region are also enriched at the intercrystalline triangular region, the oxygen content at the intercrystalline triangular region is slightly higher than that of a crystal boundary, formed oxides are increased, and after aging treatment, rare earth oxides are also distributed at the crystal boundary, so that the exchange coupling between main phases is favorably isolated, and the magnetic performance of the magnet is finally improved.

Claims (23)

1. The preparation method of the neodymium iron boron magnet material is characterized by comprising the following steps: carrying out fusion casting, hydrogen breaking, forming, sintering and aging treatment on a molten liquid of a raw material composition of the neodymium iron boron magnet material;
the neodymium iron boron magnet material comprises the following raw material compositions in percentage by mass: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent;
Cu：≥0.35%；
B：0.9~1.2%；
fe: 64-69.2%, wherein the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material;
in the intercrystalline triangular region of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element in the intercrystalline triangular region is Q1;
at the grain boundary of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element at the grain boundary is Q2;
wherein Q1 is less than Q2, and Q2 is not less than 0.1.
2. The method for preparing a neodymium-iron-boron magnet material according to claim 1, wherein the content of Pr is 17.15-26%;
and/or, the content of Nd is below 15%;
and/or, said R' also includes Y;
and/or, the R' also comprises RH which is a heavy rare earth element;
and/or the content of Cu is 0.35-1.3%;
and/or the content of B is 0.95-1.2%;
and/or the content of Fe is 64.8-69.2%;
and/or the raw material composition of the neodymium iron boron magnet material also comprises Al;
and/or the raw material composition of the neodymium iron boron magnet material also comprises Ga;
and/or the raw material composition of the neodymium iron boron magnet material also comprises Zr;
and/or the raw material composition of the neodymium iron boron magnet material also comprises Co;
and/or the raw material composition of the neodymium iron boron magnet material also comprises one or more of Zn, Ag, In, Sn, V, Cr, Mo, Ta, Hf and W.
3. The method of manufacturing a neodymium-iron-boron magnet material according to claim 2, wherein the content of Pr is 17.15%, 18.15%, 19.15%, 20.15%, 20.85%, 21.15%, 22.15%, 23.15%, 24.15%, 25.15%, or 26%;
and/or the content of Nd is 4-13%;
and/or, the RH species comprises one or more of Dy, Tb and Ho;
and/or the mass ratio of the RH to the R' is less than 0.253;
and/or the content of the RH is 1-2.5%;
and/or the Cu content is 0.35%, 0.4%, 0.45%, 0.5%, 0.6%, 0.65%, 0.7%, 0.8%, 0.85%, 0.9%, 0.95%, 1%, 1.05%, 1.1%, or 1.2%;
and/or, the content of B is 0.985%, 1%, 1.1% or 1.2%;
and/or the Fe content is 64.914%, 64.965%, 65.065%, 65.085%, 65.135%, 65.365%, 65.405%, 65.485%, 65.54%, 65.615%, 65.665%, 65.715%, 65.815%, 65.865%, 65.915%, 66.015%, 66.035%, 66.045%, 66.215%, 66.23%, 66.265%, 66.315%, 66.465%, 66.445%, 66.545%, 66.615%, 66.715%, 66.815%, 66.865%, 67.145%, 67.165%, 67.415%, 67.615%, 67.915%, 68.015%, 68.295%, 68.565% or 69.165%;
and/or when the raw material composition of the neodymium iron boron magnet material also comprises Al, the content of the Al is below 3%;
and/or when the raw material composition of the neodymium iron boron magnet material also comprises Ga, the content of the Ga is below 1%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Zr, the content of the Zr is below 0.3%;
and/or when the raw material composition of the neodymium iron boron magnet material also comprises Co, the content of the Co is 0.2-1.5%;
and/or, when the raw material composition of the neodymium iron boron magnet material further comprises Zn, the content of the Zn is below 0.1%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Mo, the content of the Mo is below 0.1%.
4. The method of manufacturing a neodymium-iron-boron magnet material according to claim 3, wherein the content of Nd is 4%, 5.85%, 6.85%, 7.85%, 8.85%, 9.85%, 10.65%, 10.85%, 11.35%, 12.35%, or 12.85%;
and/or the RH is Dy and/or Tb;
and/or the mass ratio of the RH to the R' is 0-0.07;
and/or the RH content is 1%, 1.5% or 2%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Al, the content of the Al is less than 0.5%;
and/or when the raw material composition of the neodymium iron boron magnet material also comprises Ga, the content of the Ga is 0.05-0.6%;
and/or, when the raw material composition of the neodymium iron boron magnet material further comprises Zr, the content of Zr is 0.1%, 0.2%, 0.22%, 0.25%, 0.26%, 0.27%, 0.28%, 0.29% or 0.3%;
and/or when the raw material composition of the neodymium iron boron magnet material also comprises Co, the content of the Co is 0.2% or 1%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Zn, the content of Zn is 0.04-0.08%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Mo, the content of the Mo is 0.01-0.08%.
5. The method for preparing a neodymium-iron-boron magnet material according to claim 4, wherein when the RH contains Tb, the content of Tb is 0.5-2%;
and/or, when Dy is contained in the RH, the content of Dy is 1% or less;
and/or when the RH contains Ho, the content of Ho is 0.8-2%;
and/or, when the raw material composition of the neodymium iron boron magnet material further comprises Al, the content of the Al is 0.02%, 0.03%, 0.1%, 0.2%, 0.25%, 0.3%, 0.4%, 0.45%, 0.46% or 0.48%;
and/or, when the raw material composition of the neodymium iron boron magnet material further comprises Ga, the content of the Ga is 0.1%, 0.15%, 0.18%, 0.2%, 0.24%, 0.25%, 0.3%, 0.4% or 0.5%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Zn, the content of the Zn is 0.04%, 0.05% or 0.08%;
and/or when the raw material composition of the neodymium iron boron magnet material further comprises Mo, the content of the Mo is 0.04%, 0.05% or 0.08%.
6. The method of manufacturing a neodymium-iron-boron magnet material according to claim 5, wherein when Tb is contained in the RH, the content of Tb is 0.7%, 0.8%, 0.9%, 1%, 1.5%, 1.8%, 1.9%, or 2%;
and/or, when Dy is contained in the RH, the content of Dy is 0.1%, 0.2%, or 0.3%.
7. The method for preparing the neodymium-iron-boron magnet material according to any one of claims 1 to 6, wherein the raw material composition of the neodymium-iron-boron magnet material comprises the following components in percentage by mass: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
8. The method for preparing a neodymium-iron-boron magnet material according to claim 7, wherein the content of Pr is 17.15-26% by mass of the total mass of the raw material composition of the neodymium-iron-boron magnet material;
and/or the content of Cu is 0.35-1.2%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material;
and/or, the R' also comprises RH which is a heavy rare earth element.
9. The method for preparing a neodymium-iron-boron magnet material according to claim 8, wherein when the R' further includes a heavy rare earth element, the content of the heavy rare earth element is 1-2.5%;
and/or the RH is Dy and/or Tb.
10. The method for preparing a neodymium iron boron magnet material according to claim 9, wherein when the RH further includes Tb, the content of Tb is 0.5 to 2%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material;
and/or, when the RH further comprises Dy, the content of Dy is less than 1%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
11. The method for preparing the neodymium-iron-boron magnet material according to any one of claims 1 to 6, wherein the raw material composition of the neodymium-iron-boron magnet material comprises the following components in percentage by mass: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr is more than or equal to 17.15 percent; cu: not less than 0.35 percent; al: less than or equal to 0.5 percent; ga: less than or equal to 0.42 percent; zr: 0.25 to 0.3 percent; b: 0.9-1.2%; fe: 64-69.2%; the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
12. The method for preparing a neodymium-iron-boron magnet material according to claim 11, wherein the content of Pr is 17.15-26% by mass of the total mass of the raw material composition of the neodymium-iron-boron magnet material;
and/or the content of Cu is 0.35-1.2%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material;
and/or, the R' also comprises RH which is a heavy rare earth element.
13. The method for preparing a neodymium-iron-boron magnet material according to claim 12, wherein the content of the heavy rare earth element is 1-2.5%;
and/or the RH is Dy and/or Tb.
14. The method for preparing a neodymium iron boron magnet material according to claim 13, wherein when the RH further includes Tb, the content of Tb is 0.5 to 2%, and the percentage is a mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material;
and/or, when the RH further comprises Dy, the content of Dy is less than 1%, and the percentage is the mass percentage of the total mass of the raw material composition of the neodymium iron boron magnet material.
15. The method for producing a neodymium-iron-boron magnet material according to claim 1, characterized in that grain boundary diffusion treatment is further performed after the sintering and before the aging treatment.
16. A neodymium iron boron magnet material, characterized in that it is produced by the production method according to any one of claims 1 to 15.
17. The neodymium-iron-boron magnet material is characterized by comprising the following components in percentage by mass:
r': 29.4-32.6%, wherein R' comprises Pr and Nd; wherein, the Pr is more than or equal to 17.14 percent;
Cu：≥0.34%；
B：0.9~1.2%；
Fe：64~69.2%；
the percentage is the mass percentage of the total mass of the neodymium iron boron magnet material;
in the intercrystalline triangular region of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element in the intercrystalline triangular region is Q1;
at the grain boundary of the neodymium iron boron magnet material, the ratio of the mass sum of Pr and Cu to the total mass of each element at the grain boundary is Q2;
wherein Q1 is less than Q2, and Q2 is not less than 0.1.
18. The neodymium-iron-boron magnet material as claimed in claim 17, wherein the content of Pr is 17.14-26.1%;
and/or, the content of Nd is below 15%;
and/or the ratio of the total mass of the Nd to the total mass of the R' is less than 0.5;
and/or the content of R' is 29.49-32.53%;
and/or, said R' also includes Y;
and/or R' also comprises RH which is a heavy rare earth element
And/or the content of Cu is 0.34-1.3%;
and/or the content of B is 0.95-1.2%;
and/or the content of Fe is 64.8-69.2%;
and/or, the neodymium iron boron magnet material also comprises Al;
and/or, the neodymium iron boron magnet material also comprises Zr;
and/or, the neodymium iron boron magnet material also comprises Ga;
and/or, the neodymium iron boron magnet material also comprises Co;
and/or, the neodymium iron boron magnet material also comprises O;
and/or, the neodymium iron boron magnet material also comprises one or more of Zn, Ag, In, Sn, V, Cr, Nb, Ti, Mo, Ta, Hf and W.
19. The neodymium-iron-boron magnet material of claim 18, wherein the Pr content is 17.149%, 17.15%, 17.154%, 18.15%, 18.152%, 18.154%, 18.155%, 19.15%, 19.152%, 19.154%, 19.155%, 19.159%, 20.13%, 20155%, 20.16%, 21.157%, 22.15%, 22.151%, 22.152%, 22.1555%, 23.15%, 24.151%, 24.152%, 24.155%, 24.157%, 24.158%, 25.15%, 25.152%, 25.153%, 25.156% or 26.01%;
and/or the content of Nd is 4-13%;
and/or the ratio of the total mass of the Nd to the total mass of the R' is 0.1-0.45;
and/or the R' content is 29.495%, 29.501%, 30.003%, 30.004%, 30.03%, 30.441%, 30.517%, 30.518%, 30.957%, 30.98%, 31%, 31.006%, 31.0065%, 31.009%, 31.011%, 31.012%, 31.013%, 31.498%, 31.504%, 31.539%, 31.946%, 31.972%, 31.977%, 31.995%, 31.999%, 32%, 32.001%, 32.013%, 32.015%, 32.021%, 32.022%, 32.023, 32.024%, 32.025%, 32.026%, 32.027%, 32.04%, 32.043%, 32.437% or 32.521%;
and/or, the RH species comprises one or more of Dy, Tb and Ho;
and/or the mass ratio of the RH to the R' is < 0.253;
and/or the content of the RH is 1-2.5%;
and/or the Cu content is 0.341%, 0.41%, 0.452%, 0.47%, 0.502%, 0.51%, 0.52%, 0.598%, 0.62%, 0.648%, 0.649%, 0.701%, 0.702%, 0.71%, 0.78%, 0.79%, 0.795%, 0.806%, 0.81%, 0.852%, 0.89%, 0.901%, 0.903%, 0.91%, 0.92%, 0.948%, 1.021%, 1.05%, 1.08%, 1.101%, 1.103%, 1.12%, 1.18%, 1.19%, 1.202%, or 1.21%;
and/or, the content of B is 0.983%, 0.984%, 0.985%, 0.988%, 0.989%, 1.02% or 1.19%;
and/or the Fe content is 64.965%, 65.031%, 65.095%, 65.155%, 65.204%, 65.36%, 65.4%, 65.458%, 65.525%, 65.626%, 65.63%, 65.686%, 65.817%, 65.8395, 65.869%, 65.909%, 65.963%, 65.994%, 65.995%, 66.039%, 66.04%, 66.099%, 66.157%, 66.218%, 66.267%, 66.364%, 66.377%, 66.427%, 66.437%, 66.52%, 66.605%, 66.671%, 66.8075%, 66.81%, 66.87%, 67.095%, 67.12%, 67.137%, 67.457%, 67.578%, 67.996%, 68.302%, 68.556% or 69.181%;
and/or when the neodymium iron boron magnet material further comprises Al, the content of the Al is below 0.5%;
and/or when the neodymium iron boron magnet material further comprises Zr, the content of Zr is 0.05-0.31 wt%;
and/or, when the neodymium iron boron magnet material further comprises Ga, the content of the Ga is below 0.51 percent;
and/or when the neodymium iron boron magnet material further comprises Co, the content of the Co is 0.2-1.5%;
and/or when the neodymium iron boron magnet material further comprises O, the content of the O is below 0.13%;
and/or when the neodymium iron boron magnet material further comprises Zn, the content of the Zn is 0.02-0.08;
and/or when the neodymium iron boron magnet material further comprises Mo, the content of the Mo is 0.01-0.08%.
20. The neodymium-iron-boron magnet material of claim 19, wherein the content of Nd is 4.02%, 5.847%, 5.84%, 85.849%, 5.85%, 5.851%, 5.852%, 5.853%, 5.854%, 6.851%, 6.852%, 6.853%, 7.85%, 8.846%, 8.847%, 8.85%, 8.851%, 8.852%, 8.853%, 9.85%, 9.851%, 10.844%, 10.846%, 10.849%, 11.349%, 11.384%, 12.341%, 12.345%, 12.348%, 12.35%, 12.351%, 12.364%, 12.791%, 12.802%, or 12.849%;
and/or the RH is Dy and/or Tb;
and/or the mass ratio of the RH to the R' is 0-0.07;
and/or the RH is present in an amount of 1%, 1.01%, 1.02%, 1.03%, 1.04%, 1.432%, 1.46%, 1.47%, 1.48%, 1.5%, 1.52%, 1.98%, 1.99%, 2%, 2.01% or 2.02%;
and/or when the neodymium iron boron magnet material further comprises Al, the content of the Al is 0.03-0.5 wt%;
and/or, when Zr is further included in the neodymium iron boron magnet material, the content of Zr is 0.1%, 0.21%, 0.22%, 0.25%, 0.251%, 0.252%, 0.261%, 0.272%, 0.28%, 0.281%, 0.282%, 0.291%, 0.3%, or 0.301%;
and/or when the neodymium iron boron magnet material further comprises Ga, the content of the Ga is 0.1-0.51%;
and/or, when the neodymium iron boron magnet material further comprises Co, the content of the Co is 0.2% or 1%;
and/or, when the neodymium iron boron magnet material further comprises Zn, the content of the Zn is 0.03%, 0.04% or 0.07%;
and/or, when the neodymium iron boron magnet material further comprises Mo, the content of the Mo is 0.03%, 0.06% or 0.07%.
21. The ndfeb magnet material according to claim 20, wherein the mass ratio of RH to R' is 1.01/32.015, 1.02/30.517, 1.02/32.021, 1.02/32.023, 1.02/32.024, 1.02/32.024, 1.02/32.025, 1.02/32.025, 1.02/32.026, 1.03/32.04, 1.04/32.043, 1.432/32.437, 1.46/30.441, 1.47/31.972, 1.48/31.977, 1.5/32, 1.52/32.521, 1.98/30.98, 1.99/31.995, 1/31.999, 1/32, 2.01/31.011, 2.01/31.013, 2.01/32.013, 2.02/32.022, 2.02/32.027, 2/31 or 2/31.012;
and/or, when the RH contains Tb, the content of Tb is 0.5-2 wt%;
and/or, when Dy is contained in the RH, the content of Dy is less than 0.5 wt%;
and/or when the RH contains Ho, the content of Ho is 0.8-2%;
and/or, when the neodymium iron boron magnet material further comprises Al, the Al content is 0.01%, 0.02%, 0.03%, 0.1%, 0.102%, 0.12%, 0.2%, 0.21%, 0.24%, 0.25%, 0.29%, 0.3%, 0.31%, 0.38%, 0.4%, 0.42%, 0.45%, 0.46% or 0.48%;
and/or, when the neodymium iron boron magnet material further comprises Ga, the content of the Ga is 0.1%, 0.101%, 0.102%, 0.11%, 0.12%, 0.152%, 0.18%, 0.2%, 0.202%, 0.24%, 0.25%, 0.251%, 0.302%, 0.401% or 0.501%.
22. The ndfeb magnet material as claimed in claim 21, wherein when Tb is contained in the RH, the Tb content is 0.7%, 0.72%, 0.82%, 0.9%, 0.91%, 1%, 1.02%, 1.47%, 1.48%, 1.5%, 1.81%, 1.88%, 1.89%, 1.9%, 1.91% or 2.01%;
and/or, when Dy is contained in the RH, the content of Dy is 0.1%, 0.2%, 0.21%, 0.3%, 0.31%, or 0.312%;
and/or, when the RH contains Ho, the content of Ho is 0.98%, 0.99% or 1%.
23. Use of a neodymium-iron-boron magnet material according to any one of claims 16-22 as an electronic component in an electric machine.
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ES2984871T3 (en) 2024-10-31
KR20210144906A (en) 2021-11-30
CN110828089A (en) 2020-02-21
KR102527787B1 (en) 2023-04-28

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